CN108558827A - Sulfide isobutene high pressure continuous process system and method - Google Patents
Sulfide isobutene high pressure continuous process system and method Download PDFInfo
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- CN108558827A CN108558827A CN201810751134.5A CN201810751134A CN108558827A CN 108558827 A CN108558827 A CN 108558827A CN 201810751134 A CN201810751134 A CN 201810751134A CN 108558827 A CN108558827 A CN 108558827A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D341/00—Heterocyclic compounds containing rings having three or more sulfur atoms as the only ring hetero atoms
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Abstract
A kind of sulfide isobutene high pressure continuous process system,The system includes dissolution kettle,First filter,Second filter,First flowmeter,Second flowmeter,First high-pressure pump,Second high-pressure pump,Pipeline reactor,Dissolution kettle is used for the liquefaction of solid sulfur,The pipeline reactor includes oil bath tank body,Reacting pipe,The present invention is using the reacting pipe of three-level curved structure as reactor,Reaction mass is in the continuous flowing reactive of reacting pipe,Yield can meet industrial requirement,The reacting pipe of three-level curved structure can be such that reactant is sufficiently mixed,Without mechanical agitation,The reacting pipe of three-level curved structure can make reactant form turbulent flow,The pressure stability of reacting pipe,Technology stability is high,Using single reacting pipe,Resistance to pressure is high,Reactant sulphur is reacted after liquefying in dissolution kettle,Sulphur is not will produce to distil and retaining pressure sensor,Equipment it is safe,The present invention also provides a kind of sulfide isobutene high pressure continuous producing methods.
Description
Technical field
The present invention relates to sulfide isobutene production equipment technology, more particularly to a kind of sulfide isobutene high pressure is continuously given birth to
Produce system and method.
Background technology
The production of existing sulfide isobutene has non-pressure process and high-pressure process, high-pressure process mainly to use autoclave, and high
Pressure kettle belongs to intermittent apparatus；Autoclave pressure resistance range is limited, and pressure condition stability is poor in reaction process, and product quality is unstable
It is fixed, when with autoclave produced sulfide isobutene, agitating device is needed to configure, at high temperature under high pressure, the distillation of raw material sulphur leads to magnetic
The blocking of power drive, leads to equipment fault, causes high maintenance cost, the seal structure complex of autoclave, the distillation of raw material sulphur
The blocking of sensor can be also caused stress, security risk is big.
Invention content
In view of this, against the above deficiency, it is necessary to propose it is a kind of can continuous production sulfide isobutene, high pressure, be not required to
Want mechanical agitation, pressure stability, safe sulfide isobutene high pressure continuous process system.
It is necessary to propose a kind of sulfide isobutene high pressure continuous producing method.
A kind of sulfide isobutene high pressure continuous process system, the system include dissolution kettle, first filter, the second filtering
Device, first flowmeter, second flowmeter, the first high-pressure pump, the second high-pressure pump, pipeline reactor, dissolution kettle are used for solid sulfur
Liquefaction, the entrance of the outlet of dissolution kettle and first filter connects, the outlet of first filter and the entrance of first flowmeter
Connection, the outlet of first flowmeter are connect with the entrance of the first high-pressure pump, and the entrance of the second filter is connect with isobutene storage tank,
The outlet of second filter and the entrance of second flowmeter connect, and the outlet of second flowmeter connects with the entrance of the second high-pressure pump
Connect, the pipeline reactor includes oil bath tank body, reacting pipe, and the reacting pipe is a pressure pipe, reacting pipe it is straight
Diameter is 10~50mm, and the both ends of reacting pipe are respectively reactant entrance end, product outlet end, and first high-pressure pump goes out
The outlet of mouth, the second high-pressure pump is connect with the reactant entrance end of reacting pipe, and the middle section of reacting pipe is converted into space
The zigzag part of complications trend, zigzag part are made of the zigzag section of multiple overlappings of tandem from top to down, and zigzag section is by reacting pipe
The tooth form unit for being converted into multiple arrangements that join end to end is constituted, and the zigzag part is no less than four groups, and zigzag part tandem is arranged, and mutually
It is arranged in parallel, the reaction stream in two neighboring zigzag part is submerged on the contrary, zigzag part is built in oil bath tank inner chamber vertically
In the conduction oil of oil bath tank body.
Preferably, first high-pressure pump, the second high-pressure pump are plunger pump.
Preferably, which further includes high voltage package, and the inner cavity of the high voltage package is divided by horizontally disposed high heat conduction partition board
At preheating cabinet, incubator, the first serpentine coil is set in preheating cabinet, one end of the first serpentine coil and reacting pipe it is anti-
Object arrival end is answered to connect, the other end of the first serpentine coil connects with the outlet of the first high-pressure pump, the outlet of the second high-pressure pump simultaneously
It connects, the second serpentine coil is set in incubator, the inside bottom of incubator is equipped with conduction oil, and the second serpentine coil, which is installed on, leads
More than deep fat liquid level, the feeding end of the second serpentine coil and the product outlet end of reacting pipe connect, the second serpentine coil
Discharge end is equipped with flow control valve.
Preferably, which further includes the first alembic, water washing tank, after-fractionating tank, the discharging section of the second serpentine coil
It being connect with the entrance of the first alembic, the first alembic includes that the first liquid-phase outlet, second liquid phase export, and the of the first alembic
The entrance of one liquid-phase outlet and water washing tank connects, and water washing tank includes third liquid-phase outlet, the 4th liquid-phase outlet, third liquid-phase outlet
It is connect with the entrance of after-fractionating tank, after-fractionating tank includes the 5th liquid-phase outlet, the 6th liquid-phase outlet.
Preferably, the second liquid phase outlet of first alembic is connect with the entrance of dissolution kettle.
Preferably, the top of the oil bath tank body is equipped with the first heat conducting oil inlet, and the bottom of oil bath tank body is led equipped with first
The side of hot oil outlet, incubator is equipped with the second heat conducting oil inlet, and the other side of incubator is equipped with the second conduction oil outlet, heat conduction
The outlet of oil oven is connect with the first heat conducting oil inlet, and the first conduction oil outlet is connect with the second heat conducting oil inlet, the second conduction oil
Outlet is connect with the entrance of heat-conducting oil furnace.
A kind of sulfide isobutene high pressure continuous producing method, includes the following steps：
Step 1：Solid sulfur, water are added to dissolution kettle, liquefied ammonia, hydrogen sulfide are then sequentially added, to generate ammonium polysulfide
Solution；
Step 2：Ammonium polysulfide solution, isobutene are measured respectively according to a certain percentage by first flowmeter, second flowmeter；
Step 3：Ammonium polysulfide solution, isobutene are taken by what is measured, is conveyed respectively by the first high-pressure pump, the second high-pressure pump
Enter preheating cabinet preheating, preheating temperature is higher than 90 DEG C；
Step 4：The ammonium polysulfide solution of " step 3 " preheating will be passed through, isobutene mixed liquor is sent into pipeline reactor reaction, control
Reaction temperature processed generates the solution of sulfide isobutene at 160~200 DEG C；
Step 5：The sulfide isobutene solution that reaction generates is continued to keep the temperature in incubator, holding temperature is at 160~200 DEG C；
Step 6：By by " step 5 " heat preservation after sulfide isobutene solution be sent into the first alembic distillation, separation water outlet and
Sulfide isobutene；
Step 7：Sulfide isobutene is sent into water washing tank, is washed with vulcanized sodium, cleaning solution and sulfide isobutene are isolated；
Step 8：It will be sent into after-fractionating tank redistillation by the sulfide isobutene after " step 5 " washing, high-purity sulphur is made
Change isobutene.
Preferably, it is 10~40% by the mass percent of sulphur in ammonium polysulfide solution made from " step 1 ".
Using the reacting pipe of three-level curved structure as reactor, reaction mass continuously flows the present invention in reacting pipe
Reaction, yield can meet industrial requirement, and the reacting pipe of three-level curved structure can be such that reactant is sufficiently mixed, be stirred without machinery
It mixes, the reacting pipe of three-level curved structure can make reactant form turbulent flow, and the pressure stability of reacting pipe, technology stability is high,
Using single reacting pipe, resistance to pressure is high, and reactant sulphur is reacted after liquefying in dissolution kettle, not will produce sulphur liter
China and retaining pressure sensor, equipment it is safe.
Description of the drawings
Fig. 1 is the structural schematic diagram of the sulfide isobutene high pressure continuous process system.
Fig. 2 is the structural schematic diagram of the zigzag section.
Fig. 3 is the structural schematic diagram of mixing component.
Fig. 4 is the axonometric drawing of first blender.
Fig. 5 is the upward view of second blender.
In figure：Dissolution kettle 10, mixing component 11, rotation axis 111, motor 112, the first blender 113, the first stirring rod
1131, the second blender 114, the second stirring rod 1141, first filter 20, the second filter 30, first flowmeter 40, second
Flowmeter 50, the first high-pressure pump 60, the second high-pressure pump 70, pipeline reactor 80, oil bath tank body 81, the first heat conducting oil inlet 811,
First conduction oil outlet 812, reacting pipe 82, zigzag part 821, zigzag section 8211, tooth form unit 82111, high voltage package 90, partition board
91, preheating cabinet 92, the first serpentine coil 921, incubator 93, the second serpentine coil 931, flow control valve 932, the second conduction oil
Entrance 933, the second conduction oil outlet 934, the first alembic 100, water washing tank 110, after-fractionating tank 120.
Specific implementation mode
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be apparent that, drawings in the following description are some embodiments of the invention, common for this field
For technical staff, without creative efforts, other drawings may also be obtained based on these drawings.
Referring to Fig. 1 and Fig. 2, an embodiment of the present invention provides a kind of sulfide isobutene high pressure continuous process system, the systems
Including dissolution kettle 10, first filter 20, the second filter 30, first flowmeter 40, second flowmeter 50, the first high-pressure pump
60, the second high-pressure pump 70, pipeline reactor 80, dissolution kettle 10 are used for the liquefaction of solid sulfur, the outlet of dissolution kettle 10 and first
The entrance of filter 20 connects, and the outlet of first filter 20 is connect with the entrance of first flowmeter 40, first flowmeter 40
Outlet is connect with the entrance of the first high-pressure pump 60, and the entrance of the second filter 30 is connect with isobutene storage tank, the second filter 30
Outlet connect with the entrance of second flowmeter 50, the outlet of second flowmeter 50 is connect with the entrance of the second high-pressure pump 70, pipe
Road reactor 80 include oil bath tank body 81, reacting pipe 82, reacting pipe 82 be a pressure pipe, reacting pipe 82 it is a diameter of
The both ends of 10~50mm, 500~4000m of length of reacting pipe 82, reacting pipe 82 are respectively reactant entrance end, product
Outlet end, the outlet of the first high-pressure pump 60, the outlet of the second high-pressure pump 70 are connect with the reactant entrance end of reacting pipe 82,
The middle section of reacting pipe 82 is converted into the zigzag part 821 of space complications trend, and zigzag part 821 is multiple by tandem from top to down
The zigzag section 8211 of overlapping is constituted, and zigzag section 8211 is converted into the tooth form unit of multiple arrangements that join end to end by reacting pipe 82
82111 are constituted, and zigzag part 821 is no less than four groups, and 821 tandem of zigzag part is arranged, and arranged in parallel, two neighboring zigzag part
Reaction stream in 821 is immersed in oil bath tank body 81 on the contrary, zigzag part 821 is built in 81 inner cavity of oil bath tank body vertically
In conduction oil.
Apparatus of the present invention are exclusively used in the preparation of sulfide isobutene, and sulfide isobutene, sulphur are prepared using conventional autoclave
For solid-state, and conventional pipeline reactor 80 is suitable for gas-liquid reaction, liquid-liquid reactions, using chemistry in embodiment of the present invention
Method liquefies sulphur in dissolution kettle 10, meets requirement of the pipeline reactor 80 to raw material, and the chemical method liquid used
Change, avoids method high energy consumption and high temperature melting the problem of being difficult to convey of conventional high temperature fusing.
Pipeline reactor 80 belongs to serialization equipment, and yield is big, can meet industrialization needs.
Compared with complete mixing flow stirred-tank reactor, 80 gas-liquid mixed performance of pipeline reactor is insufficient, and conventional pipeline
Mixer has baffle-type, orifice-plate type, three way type and static mixer etc., and in sulfide isobutene production, raw material ammonium polysulfide belongs to
Unstable material is susceptible to crystallization sulphur and blocks reactor.In the present invention, reacting pipe 82 uses multiple tooth form units
82111 zigzag sections 8211 for joining end to end arrangement are used as level-one tortuous, and space complications are tortuous as two level between zigzag section 8211,
Space complications form three-level complications, the three-level labyrinth arrangement of reacting pipe 82 so that turning point corner is very between zigzag part 821
Greatly, reactant forms turbulent flow by the final unstability of Multi-level deflector, meets the mixing requirement of reactant, solves conventional reactor
Using the susceptible to plugging problem of liquid phase electric hybrid module, compared with autoclave, it is no longer necessary to which special configuration mechanical agitation simplifies equipment
Structure improves the safety of equipment.
In the present invention, according to reaction needs, reacting pipe 82 is up to 500~4000m, and 82 three-level complications of reacting pipe make
The conveying of reactant needs high-pressure pump, high-pressure pump pulse to convey reactant in reacting pipe 82 so that the pressure in reacting pipe 82
Power is very unstable, to be unfavorable for the progress of reaction, and uses the three-level labyrinth arrangement of above-mentioned reacting pipe 82 so that entire anti-
It is turbulent condition to answer inner reaction tube object, and to achieve the effect that voltage stabilizing, reactant flow is uniform, when reactant is having the same
Between stop, ensure that the stabilization of product quality.
In sulfide isobutene preparation process, reaction process is exothermic reaction, and pipeline reactor 80 has temperature not in itself
Manageable disadvantage, the present invention use oil bath heating, are not in significantly overheating problem so that manifold pressure oversteps the extreme limit
Pressure, and lead to product quality accident, production process safety is more preferable, the three-level labyrinth arrangement formation of simultaneous reactions pipeline 82
Complete mixing flow reactant also provides enhanced hot transmission, further solve that 80 temperature of pipeline reactor is not easy to control and exothermic heat of reaction not
The problem of easily removing.
In the present invention, the resistance to pressure of reacting pipe 82 is very high, and especially with single pipe, intermediate sector does not connect weakness
Point, is more suitable for compressive reaction, also improves production process safety, and hyperbaric environment is conducive to the liquefaction of raw material isobutene,
The ratio for enhancing liquid-liquid reactions in reacting pipe 82 is more advantageous to and shortens the reaction time.
The first filter 20 that is arranged in the present invention, the second filter 30 can solid particle, protections first in filter stock
High-pressure pump 60, the second high-pressure pump 70 it is safe to use.
The present invention is used as reactor, reaction mass continuous in reacting pipe 82 using the reacting pipe 82 of three-level curved structure
Flowing reactive, yield can meet industrial requirement, and the reacting pipe 82 of three-level curved structure can be such that reactant is sufficiently mixed, be not necessarily to
The reacting pipe 82 of mechanical agitation, three-level curved structure can make reactant form turbulent flow, the pressure stability of reacting pipe 82, technique
Stability is high, and using single reacting pipe 82, resistance to pressure is high, and reactant sulphur is reacted after liquefaction in dissolution kettle 10,
Not will produce sulphur distillation and retaining pressure sensor, equipment it is safe.
Further, the first high-pressure pump 60, the second high-pressure pump 70 are plunger pump.
Referring to Fig. 1, further, which further includes high voltage package 90, and the inner cavity of high voltage package 90 is by horizontally disposed high heat conduction
Partition board 91 is divided into preheating cabinet 92, incubator 93, and the first serpentine coil 921, the first serpentine coil 921 are arranged in preheating cabinet 92
One end connect with the reactant entrance end of reacting pipe 82, the other end of the first serpentine coil 921 simultaneously with the first high pressure
The outlet of pump 60, the outlet connection of the second high-pressure pump 70, are arranged the second serpentine coil 931 in incubator 93, incubator 93
Inside bottom is equipped with conduction oil, and the second serpentine coil 931 is installed on heat conduction oil level or more, the pan feeding of the second serpentine coil 931
End is connect with the product outlet end of reacting pipe 82, and the discharge end of the second serpentine coil 931 is equipped with flow control valve 932.
Generally one reacting pipe 82, the first serpentine coil 921, the second serpentine coil 931 pipe.
In present embodiment, incubator 93 and preheating cabinet 92 are integrally designed, and compact-sized, preheating cabinet 92 can heat raw material
It is sent into pipeline reactor 80 afterwards, the reaction was continued in incubator 93 for the product after reaction, reaction can be made more abundant, incubator 93
Decrease the length of reacting pipe 82 to a certain extent with preheating cabinet 92.Flow control valve 932 can adjust the interior of reactor
Portion's pressure, improves safety.
Referring to Fig. 1, further, which further includes the first alembic 100, water washing tank 110, after-fractionating tank 120, and second
The discharging section of serpentine coil 931 is connect with the entrance of the first alembic 100, and the first alembic 100 includes the first liquid-phase outlet, the
First liquid-phase outlet of two liquid-phase outlets, the first alembic 100 is connect with the entrance of water washing tank 110, and water washing tank 110 includes third
Liquid-phase outlet, the 4th liquid-phase outlet, third liquid-phase outlet are connect with the entrance of after-fractionating tank 120, and after-fractionating tank 120 includes
5th liquid-phase outlet, the 6th liquid-phase outlet.
Referring to Fig. 1, further, the second liquid phase outlet of the first alembic 100 is connect with the entrance of dissolution kettle 10.
The water circulation use generated in reaction process solves the problems, such as a large amount of discharge of wastewater.
Referring to Fig. 1, further, the top of oil bath tank body 81 is equipped with the first heat conducting oil inlet 811, the bottom of oil bath tank body 81
Equipped with the first conduction oil outlet 812, the side of incubator 93 is equipped with the second heat conducting oil inlet 933, and the other side of incubator 93 is set
There is the second conduction oil outlet 934, the outlet of heat-conducting oil furnace to be connect with the first heat conducting oil inlet 811, the first conduction oil outlet 812 with
Second heat conducting oil inlet 933 connects, and the second conduction oil outlet 934 is connect with the entrance of heat-conducting oil furnace.
The present invention also provides a kind of sulfide isobutene high pressure continuous producing methods, include the following steps：
Step 1：Solid sulfur, water are added to dissolution kettle 10, liquefied ammonia, hydrogen sulfide are then sequentially added, to generate ammonium polysulfide
Solution；
Step 2：Ammonium polysulfide solution, isobutyl are measured respectively according to a certain percentage by first flowmeter 40, second flowmeter 50
Alkene；
Step 3：Ammonium polysulfide solution, isobutene are taken by what is measured, passes through the first high-pressure pump 60, the second high-pressure pump 70 respectively
Be conveyed into preheating cabinet 92 preheating, preheating temperature be higher than DEG C；
Step 4：Ammonium polysulfide solution, the feeding reaction of pipeline reactor 80 of isobutene mixed liquor of " step 3 " preheating will be passed through,
Controlling reaction temperature generates the solution of sulfide isobutene at 160~200 DEG C；
Step 5：The sulfide isobutene solution that reaction generates is continued to keep the temperature in incubator 93, holding temperature is 160~200
℃；
Step 6：It will be sent into the distillation of the first alembic 100, separation water outlet by the sulfide isobutene solution after " step 5 " heat preservation
And sulfide isobutene；
Step 7：Sulfide isobutene is sent into water washing tank 110, is washed with vulcanized sodium, isolates cleaning solution and sulfide isobutene；
Step 8：It will be sent into 120 redistillation of after-fractionating tank by the sulfide isobutene after " step 5 " washing, it is different that vulcanization is made
Butylene.
In above-mentioned " step 1 ", since hydrogen sulfide toxicity is big, sulphur, water, liquefied ammonia, hydrogen sulfide sequence are added and are based on peace
Full consideration.
In present embodiment, specifically give a kind of liquefied method of sulphur, by sequentially added in dissolution kettle 10 sulphur,
Water, liquefied ammonia, hydrogen sulfide realize the liquefaction of sulphur using chemical method, and this method is aqueous phase dissolved, compared with oil phase dissolves,
Meltage is big, and ammonia is one of the raw material that reaction is participated in during preparing sulfide isobutene, and the method overcome anti-using pipeline
Device 80 is answered to need the liquefied technical barrier of sulphur.
Further, it is 10~40% by the mass percent of sulphur in ammonium polysulfide solution made from " step 1 ".
The present invention also specifically gives a kind of mixing component 11 for above-mentioned dissolution kettle 10, which includes rotation
Axis 111, motor 112, the first blender 113, the second blender 114, rotation axis 111 stretch into from the roof of dissolution kettle 10 molten vertically
Kettle 10 inner cavity is solved, 111 upper end end of rotation axis and 112 output end of motor are coaxially connected, and 111 lower end of rotation axis is from top to down successively
First blender 113, the second blender 114 are installed, the first blender 113 is two the first stirring rod 1131, the first stirring
One end of stick 1131 is connect with the ring wall of rotation axis 111, and the other end of the first stirring rod 1131 prolongs along the radial direction of rotation axis 111
It stretches, two the first stirring rod 1131 are uniformly distributed along the circumferential direction of rotation axis 111, and the section of the first stirring rod 1131 is oval, and first
Stirring rod 1131 and the connecting pin of rotation axis 111 are fixed, and free end is reversed 45 ° and formed in an axial direction, and the second blender 114 is
The section of three the second stirring rod 1141, the second stirring rod 1141 is ellipse, and three the second stirring rod 1141 are along rotation axis 111
Circumferential direction it is uniformly distributed, one end of the second stirring rod 1141 is connect with the ring wall of rotation axis 111, the other end edge of the second stirring rod 1141
Rotation axis 111 radially extends, and is bent camber clockwise.
The shape of first blender 113, which designs, can make the flowing of the formation of the liquid phase in dissolution kettle 10 from top to down, second
The shape design of blender 114 can make the liquid phase in dissolution kettle 10 form the flowing of horizontal direction, promote in dissolution kettle 10
Liquid is sufficiently mixed, and is conducive to abundant, the fast liquefying of solid sulfur.
The steps in the embodiment of the present invention can be sequentially adjusted, merged and deleted according to actual needs.
Module or unit in device of the embodiment of the present invention can be combined, divided and deleted according to actual needs.
The above disclosure is only the preferred embodiments of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, those skilled in the art can understand all or part of the processes for realizing the above embodiment, and is wanted according to right of the present invention
Equivalent variations made by asking, still belong to the scope covered by the invention.
Claims (8)
1. a kind of sulfide isobutene high pressure continuous process system, it is characterised in that：The system include dissolution kettle, first filter,
Second filter, first flowmeter, second flowmeter, the first high-pressure pump, the second high-pressure pump, pipeline reactor, dissolution kettle are used for
The liquefaction of solid sulfur, the outlet of dissolution kettle and the entrance of first filter connect, the outlet of first filter and first flow
The entrance of meter connects, and the outlet of first flowmeter is connect with the entrance of the first high-pressure pump, the entrance and isobutene of the second filter
Storage tank connects, and the outlet of the second filter and the entrance of second flowmeter connect, the outlet of second flowmeter and the second high-pressure pump
Entrance connection, the pipeline reactor includes oil bath tank body, reacting pipe, and the reacting pipe is a pressure pipe, reaction
The both ends of a diameter of 10~50mm of pipeline, reacting pipe are respectively reactant entrance end, product outlet end, and described first is high
The outlet of press pump, the outlet of the second high-pressure pump are connect with the reactant entrance end of reacting pipe, the middle section of reacting pipe
Be converted into the zigzag part of space complications trend, zigzag part is made of the zigzag section of multiple overlappings of tandem from top to down, zigzag section by
The tooth form unit that reacting pipe is converted into multiple arrangements that join end to end is constituted, and the zigzag part is no less than four groups, zigzag part tandem row
Cloth, and it is arranged in parallel, and the reaction stream in two neighboring zigzag part is on the contrary, zigzag part is built in vertically in oil bath tank body
Chamber, and be immersed in the conduction oil of oil bath tank body.
2. sulfide isobutene high pressure continuous process system as described in claim 1, it is characterised in that：First high-pressure pump,
Second high-pressure pump is plunger pump.
3. sulfide isobutene high pressure continuous process system as claimed in claim 2, it is characterised in that：The system further includes high pressure
Packet, the inner cavity of the high voltage package is divided into preheating cabinet, incubator by horizontally disposed high heat conduction partition board, and the is arranged in preheating cabinet
The reactant entrance end of one serpentine coil, one end of the first serpentine coil and reacting pipe connects, the first serpentine coil it is another
One end is connect with the outlet of the first high-pressure pump, the outlet of the second high-pressure pump simultaneously, and the second serpentine coil is arranged in incubator, is protected
The inside bottom of incubator is equipped with conduction oil, and the second serpentine coil is installed on heat conduction oil level or more, the pan feeding of the second serpentine coil
End is connect with the product outlet end of reacting pipe, and the discharge end of the second serpentine coil is equipped with flow control valve.
4. sulfide isobutene high pressure continuous process system as claimed in claim 3, it is characterised in that：The system further includes first
Alembic, water washing tank, after-fractionating tank, the discharging section of the second serpentine coil are connect with the entrance of the first alembic, the first distillation
Tank includes the first liquid-phase outlet, second liquid phase outlet, and the first liquid-phase outlet of the first alembic and the entrance of water washing tank connect, water
Cleaning of evaporator includes third liquid-phase outlet, the 4th liquid-phase outlet, and third liquid-phase outlet is connect with the entrance of after-fractionating tank, after-fractionating
Tank includes the 5th liquid-phase outlet, the 6th liquid-phase outlet.
5. sulfide isobutene high pressure continuous process system as claimed in claim 4, it is characterised in that：First alembic
Second liquid phase outlet is connect with the entrance of dissolution kettle.
6. sulfide isobutene high pressure continuous process system as claimed in claim 5, it is characterised in that：The top of the oil bath tank body
Portion is equipped with the first heat conducting oil inlet, and the bottom of oil bath tank body is equipped with the first conduction oil outlet, and the side of incubator is led equipped with second
The other side of deep fat entrance, incubator is equipped with the second conduction oil outlet, and the outlet of heat-conducting oil furnace is connect with the first heat conducting oil inlet,
First conduction oil outlet is connect with the second heat conducting oil inlet, the entrance connection of the second conduction oil outlet and heat-conducting oil furnace.
7. a kind of sulfide isobutene high pressure continuous producing method, which is characterized in that include the following steps：
Step 1：Solid sulfur, water are added to dissolution kettle, liquefied ammonia, hydrogen sulfide are then sequentially added, to generate ammonium polysulfide
Solution；
Step 2：Ammonium polysulfide solution, isobutene are measured respectively according to a certain percentage by first flowmeter, second flowmeter；
Step 3：Ammonium polysulfide solution, isobutene are taken by what is measured, is conveyed respectively by the first high-pressure pump, the second high-pressure pump
Enter preheating cabinet preheating, preheating temperature is higher than 90 DEG C；
Step 4：The ammonium polysulfide solution of " step 3 " preheating will be passed through, isobutene mixed liquor is sent into pipeline reactor reaction, control
Reaction temperature processed generates the solution of sulfide isobutene at 160~200 DEG C；
Step 5：The sulfide isobutene solution that reaction generates is continued to keep the temperature in incubator, holding temperature is at 160~200 DEG C；
Step 6：By by " step 5 " heat preservation after sulfide isobutene solution be sent into the first alembic distillation, separation water outlet and
Sulfide isobutene；
Step 7：Sulfide isobutene is sent into water washing tank, is washed with vulcanized sodium, cleaning solution and sulfide isobutene are isolated；
Step 8：It will be sent into after-fractionating tank redistillation by the sulfide isobutene after " step 5 " washing, high-purity sulphur is made
Change isobutene.
8. sulfide isobutene high pressure continuous producing method as claimed in claim 7, it is characterised in that：It is made by " step 1 "
Ammonium polysulfide solution in sulphur mass percent be 10~40%.
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| CN113387924A (en) * | 2021-07-02 | 2021-09-14 | 新乡市瑞丰新材料股份有限公司 | Method for preparing sulfurized isobutylene by combining tail gas from hydrogen sulfide production by thiophosphoric acid |
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